CN108314001A - The preparation method of high mesoporosity charcoal - Google Patents
The preparation method of high mesoporosity charcoal Download PDFInfo
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- CN108314001A CN108314001A CN201810175286.5A CN201810175286A CN108314001A CN 108314001 A CN108314001 A CN 108314001A CN 201810175286 A CN201810175286 A CN 201810175286A CN 108314001 A CN108314001 A CN 108314001A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
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Abstract
The invention discloses a kind of preparation methods of high mesoporosity charcoal.The preparation method comprises the following steps：Sulfuric acid solution and ethyl orthosilicate are mixed, stirring obtains solution A；According to ethyl orthosilicate：Sucrose=1~4:Sucrose is added in the solution A, is stirred, obtains solution B by 1 mass ratio, and the solution B is sealed to formation gel；Gained gel is dried, later, is pre-oxidized 2~4 hours at 200~300 DEG C；Products therefrom under an inert atmosphere, is warming up to 600~900 DEG C with 5 DEG C/min, keeps constant temperature 2~4 hours, obtain carbon-silicon compound after pre-oxidizing；The carbon-silicon compound and hydrofluoric acid are mixed, stirred, is filtered, it is dry to get.Raw material sources of the present invention are extensive, environmental-friendly, product property is excellent.
Description
Technical field
The present invention relates to technical field of carbon material preparation, and in particular to a kind of preparation method of high mesoporosity charcoal.
Background technology
With the quick development of China's industry, the waste water of industrial discharge is more and more, and the waste water is usually because its structure is steady
Fixed and demurrage is long and more intractable.Wherein, the advantages that absorption method is because its is easy to operate, and effect is good and as processing industrial wastewater
Main method；Meanwhile global warming becomes one of the Tough questions that the whole world faces.Therefore, to causing its greenhouse effects
The processing of predominant gas carbon dioxide is also extremely important and urgent.Wherein, absorption method has and recycles, and energy usage is low
The advantages that, and it is a kind of effective CO2Separating treatment technology.
Porous carbon material is a kind of excellent sorbing material due to its pore structure prosperity and specific surface area high feature, makes
It has extraordinary application in terms of sewage disposal and air purification, and the key for influencing the performance of porous carbon material compares table for it
The size of face area and the structure of hole, shape etc..
Currently, the raw material for preparing porous charcoal is some timber and coal etc. mostly, not only waste of resource, but also pollution environment, and
And it is difficult to meet specific occasion at the pore structure after charcoal, shape（Such as sewage disposal makes electrode material）Demand.Cause
This, it is urgent to provide a kind of preparation methods with social and economical effects porous carbon materials.
Invention content
The high mesoporosity charcoal that the technical problem to be solved in the present invention is to provide a kind of ecologies is friendly, at low cost, has excellent performance
Preparation method.
In order to solve the above technical problems, the present invention adopts the following technical scheme that：
A kind of preparation method of high mesoporosity charcoal is designed, is included the following steps：
（1）It is 1~2mL by the amount of sulfuric acid solution and ethyl orthosilicate ratio:Sulfuric acid solution and ethyl orthosilicate are mixed, are stirred by 1g
It mixes, obtains solution A；
（2）According to ethyl orthosilicate：Sucrose=1~4:Sucrose is added to step by 1 mass ratio（1）In middle acquired solution A, into
Row stirring, obtains solution B, and the solution B is sealed to formation gel；
（3）By step（2）Middle gained gel is dried, and later, is pre-oxidized 2~4 hours at 200~300 DEG C；
（4）By step（4）Product after middle pre-oxidation is warming up to 600~900 DEG C under an inert atmosphere, with 5 DEG C/min, keeps
Constant temperature 2~4 hours, obtains carbon-silicon compound；
（5）By step（4）Gained carbon-silicon compound and hydrofluoric acid mixing, stir, filter, it is dry to get.
Preferably, in the step（1）In, the pH value of the sulfuric acid solution is 2~4.
Preferably, in the step（1）In, the stirring is magnetic agitation, and the mixing time is 2~4 h.
Preferably, in the step（3）In, drying temperature is 100~110 DEG C, and drying time is 12~30 h.
Preferably, in the step（3）In, preoxidation time is 3 h.
Preferably, in the step（4）In, constant temperature time is 3 h.
Preferably, in the step（4）In, the inert gas be in ammonia, nitrogen, hydrogen, argon gas at least
It is a kind of.
Preferably, in the step（5）In, the hydrofluoric acid be excessive, a concentration of 40% hydrofluoric acid.
Preferably, in the step（5）In, the drying time is 5~10 h.
Compared with prior art, the beneficial technical effect of the present invention lies in：
1. initiative of the invention uses sucrose（Biological source）It for carbon source, derives from a wealth of sources, is cheap, and being avoided that use
The pollution of environment and the waste of resource are caused when timber and coal.
2. the high mesoporosity charcoal prepared by the present invention has high mesoporous and specific surface area.
3. the high mesoporosity charcoal prepared by the present invention, active porosity is flourishing, and space structure shape is excellent, has very excellent
Different absorption property.
Description of the drawings
Fig. 1 is the XRD diagram of the high mesoporosity Carbon Materials prepared by embodiment 4-7；
Fig. 2 is nitrogen adsorption-desorption isotherm figure of the high mesoporosity Carbon Materials prepared by embodiment 1-4；
Fig. 3 is the graph of pore diameter distribution of the high mesoporosity Carbon Materials prepared by embodiment 1-4；
Fig. 4 is nitrogen adsorption-desorption isotherm figure of the high mesoporosity Carbon Materials prepared by embodiment 4-7；
Fig. 5 is the graph of pore diameter distribution of the high mesoporosity Carbon Materials prepared by embodiment 4-7；
Fig. 6 is the canonical plotting of methylene blue solution.
Specific implementation mode
Illustrate the specific implementation mode of the present invention with reference to the accompanying drawings and examples, but following embodiment is used only in detail
It describes the bright present invention in detail, does not limit the scope of the invention in any way.
Involved instrument and equipment is routine instrument device unless otherwise instructed in the examples below；Involved
Material and reagent are purchased from conventional chemical reagent shop unless otherwise instructed；Involved test, preparation method, such as without especially
Illustrate, is conventional method.
The preparation of 1 high mesoporosity charcoal of embodiment
The sulfuric acid that 6 mL pH are 2 is first added into conical flask, then adds 4 g ethyl orthosilicates（TEOS）, later will dress
There is the conical flask of the sulfuric acid and ethyl orthosilicate to be placed on magnetic stirring apparatus, 3 h of stirring so that solution is in transparent and homogeneous, then
4 g sucrose are weighed, are added in the conical flask, continuing stirring makes the sucrose be completely dissolved, later, by the mixed liquor of formation
It pours into test tube, seals, make its gel.
After homogeneous and transparent gel to be formed, the test tube equipped with the gel is smashed, gel is taken out and is put into beaker, into
Row drying.Gel after drying is pre-oxidized 3 hours for 250 DEG C in Muffle furnace, then in N2Under atmosphere, heated up with 5 DEG C/min
To 900 DEG C, constant temperature 3 hours is carbonized, and rear Temperature fall obtains carbon-silicon compound.
By the carbon-silicon compound with excessive 40% hydrofluoric acid（HF）16 h are stirred, are filtered, later, in 100 DEG C of dryings
8 h obtain high mesoporosity Carbon Materials.The high mesoporosity charcoal is denoted as SAC-1-900, wherein 1 indicates ethyl orthosilicate and sugarcane
The mass ratio of sugar, 900 indicate carbonization temperature.
The preparation of 2 high mesoporosity charcoal of embodiment
As different from Example 1：The quality of ethyl orthosilicate is 8 g, i.e., the mass ratio of ethyl orthosilicate and sucrose is 2,
Remaining is same as Example 1.Resulting materials are denoted as SAC-2-900.
The preparation of 3 high mesoporosity charcoal of embodiment
As different from Example 1：The quality of ethyl orthosilicate is 12 g, i.e., the mass ratio of ethyl orthosilicate and sucrose is 3,
Remaining is same as Example 1.Resulting materials are denoted as SAC-3-900.
The preparation of 4 high mesoporosity charcoal of embodiment
As different from Example 1：The quality of ethyl orthosilicate is 16 g, i.e., the mass ratio of ethyl orthosilicate and sucrose is 4,
Remaining is same as Example 1.Resulting materials are denoted as SAC-4-900.
The preparation of 5 high mesoporosity charcoal of embodiment
As different from Example 3：Carbonization temperature is 800 DEG C, remaining is same as Example 3.Resulting materials are denoted as SAC-
3-800。
The preparation of 6 high mesoporosity charcoal of embodiment
As different from Example 3：Carbonization temperature is 700 DEG C, remaining is same as Example 3.Resulting materials are denoted as SAC-
3-700。
The preparation of 7 high mesoporosity charcoal of embodiment
As different from Example 3：Carbonization temperature is 700 DEG C, remaining is same as Example 3.Resulting materials are denoted as SAC-
3-600。
The Char Yield of high mesoporosity charcoal product prepared by 8 embodiment 1-7 of embodiment
Char Yield such as the following table 1 of product prepared by the embodiment 1-7, wherein Char Yield is gained high mesoporosity charcoal
The quality of sucrose after quality/pre-oxidation.
。
Embodiment 9 carries out XRD tests to the high mesoporosity Carbon Materials prepared by embodiment 4-7
Use the instrument model of German Bruker companies production made to embodiment 5-7 for the X-ray diffractometer of D8 ADVANCE
Standby Carbon Materials carry out XRD tests.Test condition is 35 kV of voltage, and the range of scan angle is 10~90 °.
Attached drawing 1 is the XRD test results of high mesoporosity Carbon Materials obtained by embodiment 5-7, is implemented it can be seen from attached drawing 1
The microstructure of high mesoporosity Carbon Materials prepared by example 5-7 is agraphitic carbon structure.
Embodiment 10 carries out specific surface area and opening size test to the high mesoporosity charcoal prepared by embodiment 1-7
The specific surface area pore size determination instrument of the 2QDS-MP-30 produced using Kang Ta instrument companies of the U.S. carries out specific surface area and hole
Diameter is tested.High mesoporosity charcoal prepared by 50 mg embodiments 2-9 is weighed, in 250 DEG C of 12 h of vacuum outgas.Utilize Brunauer-
Emmett-Teller（BET）Method calculates the specific surface area of material, and micropore specific area and porous body are calculated with t-plot methods
Product, with BJH theory analysis pore-size distributions.
The adsorption/desorption isotherms such as attached drawing 2 of high mesoporosity Carbon Materials prepared by embodiment 1-4, graph of pore diameter distribution such as attached drawing
3；The adsorption/desorption isotherms such as attached drawing 4 of high mesoporosity Carbon Materials prepared by embodiment 4-7；Graph of pore diameter distribution such as attached drawing 5.
From attached drawing 3,5 it will be evident that the aperture of the high mesoporosity Carbon Materials prepared by embodiment 1-7 is with mesoporous
Main, aperture is mainly distributed between 2.5 nm to 6 nm.
Pass through the N of attached drawing 2 and attached drawing 42The pore structure parameter of the calculated sample of adsorption-desorption isothermal, embodiment 1-7
Pore structure parameter such as the following table 2 of prepared high mesoporosity Carbon Materials.
。
It can be seen that from upper table 2, the high mesoporosity Carbon Materials prepared by embodiment 1-7 have big specific surface area and hole body
Product.
Embodiment 11 carries out absorption property test to the high mesoporosity charcoal prepared by embodiment 1-7
The methylene blue that 10 mg are weighed on electronic balance is placed in the volumetric flask of 100 mL；Then plus distilled water is to scale
Line is configured to the methylene blue solution of a concentration of 100 mg/L.The methylene blue solution of a concentration of 100 mg/L is diluted respectively
For the standard solution of the various concentrations such as 1 mg/L, 2 mg/L, 3 mg/L, 4 mg/L, 5 mg/L, 6 mg/L, its suction is then tested
Methylene blue standard curve is made, such as attached drawing 6 in luminosity.
The high mesoporosity Carbon Materials prepared by 10 mg embodiments 1-7 are weighed respectively to be placed in the conical flask of 50 mL, then are divided
The methylene blue solution of a concentration of 50 mg/L of 20 mL is not added, shakes 20 min at room temperature, takes supernatant liquor, is put into centrifugation
Machine centrifuges, and takes the supernatant liquor after centrifugation to measure its absorbance with spectrophotometric, then calculates its adsorbance, as a result such as the following table 3.
。
The present invention is described in detail above in conjunction with drawings and examples, still, those of skill in the art
Member is it is understood that without departing from the purpose of the present invention, can also carry out each design parameter in above-described embodiment
Change, forms multiple specific embodiments, is the common variation range of the present invention, is no longer described in detail one by one herein.
Claims (9)
1. a kind of preparation method of high mesoporosity charcoal, includes the following steps：
（1）By 1~2mL:The amount ratio of 1g takes sulfuric acid solution, ethyl orthosilicate to be mixed, and obtains solution A；
（2）By ethyl orthosilicate：Sucrose=1~4:1 mass ratio takes sucrose to be added in the solution A, is obtained after mixing
Solution B seals the solution B until forming gel；
（3）By step（2）Middle gained gel is dried, and later, is pre-oxidized 2~4 hours at 200~300 DEG C；
（4）By the product after pre-oxidation obtained by upper step under indifferent gas atmosphere, 600~900 are warming up to the rate of 5 DEG C/min
DEG C, and keep constant temperature 2~4 hours, obtain carbon-silicon compound；
（5）Again to by step（4）Excessive hydrofluoric acid is added in gained carbon-silicon compound, is mixed, filters, it is dry solid remaining
Object to get.
2. the preparation method of high mesoporosity charcoal according to claim 1, which is characterized in that in the step（1）In, it is described
The pH value of sulfuric acid solution is 2~4.
3. the preparation method of high mesoporosity charcoal according to claim 1, which is characterized in that in the step（1）In, it is described
Stirring is magnetic agitation, and the mixing time is 2~4 h.
4. the preparation method of high mesoporosity charcoal according to claim 1, which is characterized in that in the step（3）In, it is dry
Temperature is 100~110 DEG C, and drying time is 12~30 h.
5. the preparation method of high mesoporosity charcoal according to claim 1, which is characterized in that in the step（3）In, pre- oxygen
The change time is 3 h.
6. the preparation method of high mesoporosity charcoal according to claim 1, which is characterized in that in the step（4）In, constant temperature
Time is 3 h.
7. the preparation method of high mesoporosity charcoal according to claim 1, which is characterized in that in the step（4）In, it is described
Indifferent gas is at least one of ammonia, nitrogen, hydrogen, argon gas.
8. the preparation method of high mesoporosity charcoal according to claim 1, which is characterized in that in the step（5）In, it is described
Hydrofluoric acid weight percent concentration is 40%.
9. the preparation method of high mesoporosity charcoal according to claim 1, which is characterized in that in the step（5）In, it is described
Drying time is 5~10 h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810175286.5A CN108314001B (en) | 2018-03-02 | 2018-03-02 | Preparation method of high and medium porosity carbon |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810175286.5A CN108314001B (en) | 2018-03-02 | 2018-03-02 | Preparation method of high and medium porosity carbon |
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| Publication Number | Publication Date |
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| CN108314001A true CN108314001A (en) | 2018-07-24 |
| CN108314001B CN108314001B (en) | 2021-06-15 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1899959A (en) * | 2006-07-19 | 2007-01-24 | 中国石油化工股份有限公司 | Method for preparing ordered mesoporous carbon |
| CN101362598A (en) * | 2008-08-27 | 2009-02-11 | 暨南大学 | Synthetic process of ordered mesoporous carbon material |
| CN102897748A (en) * | 2012-10-29 | 2013-01-30 | 中国石油大学(华东) | Method for preparing high-mesoporosity starch-based mesoporous carbon |
| CN103482596A (en) * | 2012-06-12 | 2014-01-01 | 北京化工大学 | Preparation method and application of ordered mesoporous carbon |
| US20170001153A1 (en) * | 2013-11-29 | 2017-01-05 | National Institute For Materials Science | Nanofiltration or reverse osmosis membrane made of hard carbon film, filtering filter, two-layer-bonded-type filtering filter, and methods for manufacturing same |
-
2018
- 2018-03-02 CN CN201810175286.5A patent/CN108314001B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1899959A (en) * | 2006-07-19 | 2007-01-24 | 中国石油化工股份有限公司 | Method for preparing ordered mesoporous carbon |
| CN101362598A (en) * | 2008-08-27 | 2009-02-11 | 暨南大学 | Synthetic process of ordered mesoporous carbon material |
| CN103482596A (en) * | 2012-06-12 | 2014-01-01 | 北京化工大学 | Preparation method and application of ordered mesoporous carbon |
| CN102897748A (en) * | 2012-10-29 | 2013-01-30 | 中国石油大学(华东) | Method for preparing high-mesoporosity starch-based mesoporous carbon |
| US20170001153A1 (en) * | 2013-11-29 | 2017-01-05 | National Institute For Materials Science | Nanofiltration or reverse osmosis membrane made of hard carbon film, filtering filter, two-layer-bonded-type filtering filter, and methods for manufacturing same |
Non-Patent Citations (1)
| Title |
|---|
| 栾光贵 等: ""模板法中孔炭材料的制备与表征"", 《炭素技术》 * |
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